The first report of using limonene derivative of a spherosilicate as a modifier of polylactide used for 3D printing and injection moulding is presented. The paper presents the use of limonene-functionalized spherosilicate derivative as a functional additive. The study compared the material characteristics of polylactide modified with SS-Limonene (0.25–5.0% w/w) processed with traditional injection moulding and 3D printing (FFF, FDM). A significant improvement in the processing properties concerning rheology, inter-layer adhesion, and mechanical properties was achieved, which translated into the quality of the print and reduction of waste production. Moreover, the paper describes the elementary stages of thermal transformations of the obtained hybrid systems.
The fractionation of diatomaceous earth (DE) using sedimentation made it possible to obtain separate unbroken diatom fractions from broken or agglomerated bodies with a range of particle sizes. The produced filler was used to prepare polylactide (PLA)/diatomaceous earth biocomposite samples containing different particle sizes, which were subjected to mechanical testing (tensile strength, flexural strength, impact strength), colloidal testing (contact angle, color change test, SEM/EDS), and thermal testing (TGA, DSC, DMA). Modification of the PLA containing the smallest particle size with diatomaceous earth (Fraction 5) resulted in a higher impact strength compared to both the pure PLA and the PLA/DE composite that contained base diatomaceous earth. Furthermore, the melt flow rate was improved by more than 80 and 60% for the composite modified with fractionated diatomaceous earth (Fraction 4) compared to pure PLA and base diatomaceous earth, respectively. The elasticity of the composite was also improved from 3.3 GPa for pure polylactide to 4.4 GPa for the system containing the smallest diatomaceous earth particles (Fraction 5).
This publication summarises the current state of knowledge and technology on the possibilities and limitations of using mineral and synthetic fillers in the field of 3D printing of thermoplastics. FDM technology can be perceived as a miniaturised variation of conventional extrusion processing (a microextrusion process). However, scaling the process down has an undoubtful drawback of significantly reducing the extrudate diameter (often by a factor of ≈20–30). Therefore, the results produced under conventional extrusion processing cannot be simply translated to processes run with the application of FDM technology. With that in mind, discussing the latest findings in composite materials preparation and application in FDM 3D printing was necessary.
In this work, silsesquioxane and spherosilicate compounds were assessed as novel organosilicon coupling agents for surface modification of TiO2 in a green process, and compared with their conventional silane counterparts. The surface-treated TiO2 particles were then applied in preparation of epoxy (EP) composites and the aspects of pigment dispersion, suspension stability, hiding power, as well as the composite mechanical and thermal properties were discussed. The studied compounds loading was between 0.005–0.015% (50–150 ppm) in respect to the bulk composite mass and resulted in increase of suspension stability and hiding power by over an order of magnitude. It was found that these compounds may be an effective alternative for silane coupling agents, yet due to their low cost and simplicity of production and manipulation, silanes and siloxanes are still the most straight-forward options available. Nonetheless, the obtained findings might encourage tuning of silsesquioxane compounds structure and probably process itself if implementation of these novel organosilicon compounds as surface treatment agents is sought for special applications, e.g., high performance coating systems.
We report here functionalizing borasilsesquioxanes in a cross‐metathesis reaction in the presence of a ruthenium catalyst. The procedure provides new, silsesquioxanes containing boron atoms in their structure, which may find potential application in the preparation of special materials, e.g. flame retardants for polymers, organoboron Lewis acids for catalysts and scavengers, or molecular probes. The most attractive aspect of this study was obtaining hybrid silsesquioxane systems in the metathesis reaction of styrylborasilsesquioxane with mono‐ and octavinylsilsesquioxanes as well as diborate systems with vinylborate derivatives. Most of the compounds were obtained in good yields (> 75 %) and were characterized by spectroscopic methods (NMR, MALDI‐TOF‐MS).
In this work, a seriTables of silsesquioxanes (SSQ) and spherosilicates (SS), comprising a group of cage siloxane (CS) compounds, was tested as functional additives for preparation of isotactic polypropylene (iPP)-based nanocomposites and discussed in the aspect of their rationale of applicability as such additives. For this purpose, the compounds were prepared by condensation and olefin hydrosilylation reactions. The effect of these cage siloxane products on properties of obtained CS/iPP nanocomposites was analyzed by means of mechanical, microscopic (scanning electron microscopy-energy dispersive spectroscopy), thermal (differential scanning calorimetry, thermogravimetry), thermomechanical (Vicat softening point) analyses. The results were compared with the previous findings on CS/polyolefin composites. The role of CS compounds was discussed in terms of plastic processing additives.
The presented work is a continuation of research on the reactivity of unsaturated borasilsesquioxanes under the conditions of common organometallic transformations. The catalytic hydrosilylation reaction with silanes, siloxanes and silsesquioxanes in presence of platinum catalyst was explored. The majority of the products were obtained in high yields (> 90 %) and their structures were confirmed and characterized by spectroscopy and spectrometry, i. e. NMR and MALDI-TOF-MS.The most significant segment of the work is research on the spontaneous redistribution reaction of the alkoxy group from silane to borane moiety occurring in the obtained products, not being limited to the heterosilsesquioxane chemistry, however. The products were confirmed using GC-MS, ESI-MS methods and B3LYP exchange-correlation, in order to ascertain formation of the silicon-boron hybrid molecule.
The functionalization of mono- and octahydrospherosilicate with vinylboranes and allylboranes via hydrosilylation reaction in the presence of a Karstedt’s platinum (0) catalyst is presented. This is the catalytic route to obtain a new class of silsesquioxanes containing boron atoms in their structure in high yields (>90%) and with satisfactory selectivity. The obtained compounds were fully characterized by spectroscopic (1H, 13C, 29Si NMR) and spectrometric methods (MALDI-TOF-MS), as well as thermal analysis (TGA). The obtained compounds were subjected to thermal tests, characterizing the processes of melting, thermal evaporation, sublimation and thermal decomposition.
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